Establishment of the detection method for the adulteration of Bupleurum marginatum in Ganmao qingre granules and determination of adulteration limit
- VernacularTitle:感冒清热颗粒中藏柴胡掺伪检测方法的建立及掺伪限度拟定
- Author:
Dantong ZHAO
1
;
Yijun GAO
2
;
Tianchen BI
3
;
Jinghua LIU
3
;
Weikun ZHU
3
;
Suxiang WANG
3
;
Rong RONG
4
Author Information
1. Heze Institute for Food and Drug Control，Shandong Heze 274000，China;College of Pharmacy，Shandong University of Traditional Chinese Medicine，Jinan 250355，China
2. Dept. of Pharmacy，Heze Municipal Hospital，Shandong Heze 274031，China
3. Heze Institute for Food and Drug Control，Shandong Heze 274000，China
4. College of Pharmacy，Shandong University of Traditional Chinese Medicine，Jinan 250355，China
- Publication Type:Journal Article
- Keywords:
Ganmao qingre granules;
Bupleurum marginatum;
nepasaikosaponin K;
adulteration;
HPLC-MS/MS
- From:
China Pharmacy
2022;33(20):2454-2459
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE To establish the de tection method for the adulteration of Bupleurum marginatum in Ganmao qingre granules，and to determine the adulteration limit . METHODS HPLC-MS/MS method was used to detect the content of nepasaikosaponin K in commercial and self -made samples of Ganmao qingre granules ，using electrospray ionization ，and the analysis was carried out under multiple reaction monitoring model in negative mode with m/z 943.6→635.5 as the quantitative ion pair. The calculation method was established for the adulteration proportion of B. marginatum in Ganmao qingre granules . Taking nepasaikosaponin K as the index ，the adulteration limit was determined . RESULTS The linear range of nepasaikosaponin K were 0.051-20.200 μg/mL（r＝0.999 1）. RSDs of precision ，repeatability and stability （24 h）tests were all lower than 2.50%. The average recoveries were 97.58%（RSD＝2.09%，n＝9）. The limit of detection was 0.60 μg/g，the limit of quantitation was 1.80 μg/g. The adulteration ratio of B. marginatum in Ganmao qingre granules had a good linear relationship to the peak area of nepasaikosaponin K in the range of 5%-100%（r＝0.990 9）. The contents of nepasaikosaponin K in 15 batches of Ganmao qingre granules were 2.584-56.661 μg/g. One batch of samples exceeded the proposed adulteration limit （10%），and the unqualified rate was 6.67%. CONCLUSIONS The established analytical method can be used to detect the adulteration of B. marginatum in Ganmao qinggre granules ，the proposed adulteration limit is 10%.
